12.0 sampling methods requirements - biosystems … detection limit is 0.01 ppm for a 0-10 ppm...

A Quality Assurance Project Plan for Monitoring Gaseous and Particulate Matter Emissions from Broiler Housing Section No.: 12

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12.0 Sampling Methods Requirements These methods provide for continuous measurement of the gas concentration, particulate matter concentration, ventilation rate, environmental conditions, DAQ recording and litter samples.

12.1 Gas Concentration Analysis Methods Ammonia The NH3 concentrations of background and exhaust air are measured with an advanced photo-acoustic, highly accurate, responsive and stable NH3 analyzer. This type of analyzer has been widely used by European and Japanese scientists and recently used by U.S. scientists in AFO air emission studies (Battye, 1994). The sampling interval of the advanced INNOVA 1412 photo-acoustic multi-gas analyzer is set at 30 second per sample for measuring three different air pollutants (NH3, CO2, non-methane hydrocarbons) with three individual optical filters (INNOVA filter number: 976, 983, 987 for NH3, CO2 and NMHC respectively). The low detection limit for NH3 is 0.2 ppm with up to 2,000 ppm maximum range. The response time of the INNOVA 1412 is shorter than four sampling cycles (30 s × 4 = 120 s) described in Appendix D. In addition, two Drager Polytron I electro-chemical ammonia monitoring units (at location SW1 and TE1 are used as a backup for NH3 monitoring. Hydrogen Sulfide Advanced Pollution Instrumentation, Inc., Model 101E H2S analyzer is being used to measure the H2S concentrations of background and exhaust air. The detection limit of the analyzer is 0.4 ppb with maximum range 20,000 ppb. The response time of T95 for both rising and falling is shorter than 100 sec, which was tested in the lab (see Appendix K and API 101E instruction manual). T95 is defined as the time it takes for the instrument to respond to 95% of a chosen concentration when the initial concentration is zero or background air. Non-Methane Hydrocarbons The VIG Industries, Inc. Model-200 is a microprocessor-based, dual-channel, oven heated methane/non-methane/total hydrocarbon gas analyzer. Designated for use as USEPA Method 18 and Method 25A, it measures total hydrocarbons and methane and non-methane components (VOC) of background and exhaust air (Appendix L). The detection limit is 0.01 ppm for a 0-10 ppm range. Total hydrocarbon is continuously measured with a less than 5-second response time of T90. T90 is defined as the time it takes for the instrument to respond to 90% of a chosen concentration when the initial concentration is zero or background air. Methane and non-methane hydrocarbon are measured and updated every three minutes. Carbon Dioxide The CO2 concentrations of background and exhaust air are measured with an advanced photo-acoustic, highly accurate, responsive and stable multi-gas analyzer. The sampling frequency of the advanced INNOVA 1412 photo-acoustic analyzer was set at 30 second/sample for measuring three different air pollutants (NH3, CO2, non-methane hydrocarbon) with three individual optical filters. The low detection limit for CO2 is 3.4 ppm with up to 34,000 ppm maximum range. The response time of the INNOVA 1412 is shorter than four sampling cycles (30 s × 4 = 120 s).

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Lara B. Moody, Hong Li, Robert T. Burns, Hongwei Xin, Richard S. Gates, Steven J. Hoff, Doug Overhults. 2008. Sections 12-17, pp. 63-102 in A Quality Assurance Project Plan for Monitoring Gaseous and Particulate Matter Emissions. Copyright © American Society of Agricultural and Biological Engineers. ASABE # 913C0708e.


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of 11 12.2 Gas Sampling Collection and Preparation Individual air samples, as defined in Section 11, for both in-house and background locations are collected using a gas sampling system (GSS) that is designed to collect samples from four locations on a cyclical basis. Three sampling points are located inside each broiler house at two sidewall fans and at the tunnel end. The fourth sampling point is located outside of the broiler house and is used as the ambient measurement point for background concentration determination. The location of the sampling points in Tyson 1-5 and Tyson 3-3 are shown in Figure 11.1. The samples are pumped into the GSS with pumps on the inlet side of the GSS. This arrangement results in the GSS being a positive pressure system. By using this positive pressure approach, if a leak were to develop at any connection point on the GSS it cannot compromise the integrity of the gas sample. A more detailed description of the GSS is provided below and in Appendix B: SOP of GSS. 12.3 Gas Sampling Equipment, Preservation and Handling Time Requirements Vacuum pumps (P1-P4) with Teflon wetted parts will be used to deliver air from the sampling locations via solenoids and a manifold (M1), and then transport the air stream to another manifold (M2) connected to the gas analyzer. Teflon or Teflon coating will be used in all wetted parts of the sampling system (pump, solenoid valves, manifold, and tubing). Four pairs of 2-way solenoid valves (S1-S8) located in sampling lines are controlled by the DAQ and control unit to allow measurements of gas concentrations by automatic gas sampling from four locations (Figure 11.3). To avoid the malfunction of solenoid valves as a result of overheating, solenoid cool boards are used to drive the solenoid valves. When the control module sends the signal to the cool boards, the cool boards provide full power (12 VDC) to the solenoids during the first 100 milliseconds and then cut the power to approximately half (5 VDC) and hold it for 120 or 480 seconds until the DAQ system receives the fourth output signal from INNOVA 1412 analyzer via RS232. The cool boards solve the overheating problem of the solenoid valves. Individual supply pumps with 16 L/min delivering capacity are used to continuously draw air from each of the sampling locations. The sampling train is designed such that samples are drawn from all four sampling points continuously. When a sampling point is not being analyzed, the flow is bypassed through the normally open solenoid valve (S5-S8). This arrangement is designed to minimize the residence time and greatly reduce the sample-to-sample purging time. When a sampling stream is selected, the corresponding normal close valve will open and the normal open valve will close, and the selected gas stream will flow from the sample inlet via the tubing through the manifolds (M1 and M2). The internal pump of the gas analyzers draws air from manifold M2. The gas sampling system is designed such that all solenoid valves, manifolds, and associated connections are under positive pressure. Using this positive pressure approach, if a leak were to develop on the gas sampling control board at any of these components, it would not impact the integrity of the gas sample. Two pleated paper filters enclosed in plastic, then shrouded in screen wire are used to exclude coarse debris from entering the sample lines. Additionally, a 47-mm diameter, in-line Teflon

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of 11 PFA filter holder housing a 47-mm diameter, Teflon PTFE-laminated polypropylene membrane filter with 20-μm pore size is installed at the sampling end of each gas sampling tube to remove airborne particulate from the sampled air (Figure 12.1). Another 5-μm pore size PTFE filter is installed after the vacuum pump to provide double protection. The in-house sample-point, intake filters are changed weekly and the in-line, 20- μm filter is changed at the midpoint and at the end of the flock grow out period.

Figure 12.1. Photographs of the air sampling system.

All portions of the sample tubing that go from a warm area to, or thru, a cooler area is heat traced to a temperature of 120°F to maintain a temperature well above dew point in order to prevent in-line condensation. The GSS is heat traced and maintained at 100°F to avoid any condensation in the system. Temperature of the sampling line and the power input of the heat trace or tape is continuously monitored and regulated through the DAQ and control system. Gas samples are analyzed using an INNOVA 1412 Photoacoustic Multi-Gas Monitor with RS232 output, API 101E UV Fluorescence H2S Analyzer and Non-Methane hydrocarbon using VIG200 methane/non-methane/total hydrocarbon analyzer and the INNOVA 1412 (Figure 11.3). Because the INNOVA 1412 has a separate filter for each analyzed component, it can continuously monitor five pollutants. For more details on the operation and specifics for the INNOVA 1412 (NH3, CO2, non-methane hydrocarbon), see Appendix D. The INNOVA 1412 is specified with 1-second sampling integration time and a fixed flushing time (chamber-2 seconds and tubing-3 seconds). Using a 30-second measurement cycle, the INNOVA demonstrates a T95-97 response time of 120 seconds (i.e., four measurement cycles), see Appendix D. Hence, the first 2-3 readings during each sampling period are considered invalid and excluded in the determination of the emission rate. The volume of sample air is 100cm3/sample. The INNOVA 1412 sampling flow rate is 1.8 L/min. The response time of the API 101E UV Fluorescence H2S Analyzer to step changes in gas concentrations was tested. For more details on the operation and specifics for the API 101E UV Fluorescence H2S Analyzer, see Appendix K. The response time of the API 101E is shorter than 100 seconds. The API 101E sampling flow rate is 0.6 L/min. The VIG model 200 methane/non-methane/total hydrocarbon analyzer uses column technology to separate methane and non-methane from total hydrocarbons and uses a dual FID (flame

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of 11 ionization detectors) to measure each component in the air sample. The VIG model 200 sampling flow rate is 2.5-3.0 L/min. To obtain continuous gas data to match continuous airflow, the data in long intervals between valid readings is estimated by linear interpolation, as described in Section 11.1. The air sampling schedule from four locations is determined by the fan running status at three inside locations. Table 12.1 summarizes the sampling methods and intervals for easy reference.

Table 12.1. Gas sampling locations and sampling methods/SOPs. Sampling location

Sidewall fan 1

Sidewall fan 3 Tunnel end Outside

Location ID Number 1 2 3 0

Analytical Parameters

NH3, CO2, H2S, NMHC,

and CH4 (ppm)

NH3, CO2, H2S, NMHC,

and CH4 (ppm)

NH3, CO2, H2S,

NMHC, and CH4 (ppm)

NH3, CO2, H2S,

NMHC, and CH4 (ppm)

Sampling SOP Appendix B, D, G, K, and L

Appendix B, D, G, K, and L



Sample Flow Rate 15 L/min 15 L/min 15 L/min 15 L/min Sampling Time 120 s 120 s 120 s 480 s

No Fan 120 s 2 hr SW 1 or 2 120 s 2 hr SW 3 or 4 120 s 2 hr

Any Tunnel Fan (TF) 120 s 2 hr SW 1 or 2 + SW 3 or 4 240 s 240 s 2 hr

SW 1 or 2 + any TF 240 s 240 s 2 hr SW 3 or 4 + any TF 240 s 240 s 2 hr

Exhaust Fans Running

Combinations

SW 1 or 2 + SW 3 or 4 + any TF 360 s 360 s 360 s 2 hr

12.4 Particulate Matter Concentration Methods TSP The TSP mass concentration of the exhaust air is measured by the Rupprecht & Patashnick TEOM series 1400a PM10 monitor (Appendix M) designated as Reference Method number EQPM-1090-79 as per 40 CFR Parts 58. For measuring TSP, the PM10 inlet will be replaced by a TSP inlet. The TEOM 1400a is a true gravimetric instrument that draws ambient air through a filter at a constant flow rate, continuously weighting the filter and calculating near real-time (2 sec) mass concentration. The mass concentration is calculated by the exponential smoothing based on the total mass loaded on the filter. The TSP TEOM is operated in the house with a flow rate of 16.7 L/min (1 L/min main flow and 15.67 L/min auxiliary flow); the total mass and mass rate/mass concentration averaging times are set at 300 seconds; the temperature of the sample stream will be set at 50 C. The mass concentration unit of ug/m3 is used. The output of the mass

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of 11 concentration is based on a standard temperature and pressure of 25°C and 1 atmosphere (atm), respectively. PM10 The PM10 mass concentration of the exhaust air is measured by the Rupprecht & Patashnick TEOM series 1400a PM10 monitor (Appendix N) designated as Reference Method number EQPM-1090-79 as per 40 CFR Parts 58. The TEOM 1400a is a true gravimetric instrument that draws ambient air through a filter at a constant flow rate, continuously weighing the filter and calculating near real-time (2 second) mass concentration. The mass concentration is calculated by the exponential smoothing based on the total mass loaded on the filter. The PM10 TEOM is operated in the house with a flow rate of 16.7 L/min (1 L/min main flow and 15.67 L/min auxiliary flow). The total mass and mass rate/mass concentration averaging times are set at 300 seconds. The temperature of the sample stream is set at 50°C. The mass concentration unit of ug/m3 is used. The output of the mass concentration is based on a standard temperature and pressure of 25°C and 1 atmosphere (atm), respectively. PM2.5 The PM2.5 mass concentration of the exhaust air is measured with the Rupprecht & Patashnick TEOM series 1400a PM10 monitor (Appendix O) with the addition of the PM2.5 cyclone designated as Reference Method number EQPM-1090-79 as per 40 CFR Parts 58. The PM2.5 TEOM is operated in the house with a flow rate of 16.7 L/min, with the total mass and mass rate/mass concentration averaging times set at 300 seconds. The detection limit of the TEOM is 0.01 ug/m3. TEOM is a USEPArecognized, correlated acceptable continuous monitor for continuous PM2.5 measurements. TSP, PM10 and PM2.5 TEOMs are placed in the houses at location SW1 or tunnel end (Figures 11.1 and 11.2). The analog outputs (mass concentration, pressure drop percentage and auxiliary flow rate) from TSP, PM10 and PM2.5 TEOMs will be connected to and recorded by Compact Fieldpoint. With the fan flow rate from fan runtime monitoring and calibrated fan curve, the particulate matter emission will be calculated (see Appendix J). During the brooding period, the TEOMs are placed at SW1 sampling location. When the brood curtain is open, the TEOMs are moved to the tunnel end sampling location. Because of the intermittent fan operation in broiler houses it is critical that PM concentration be correlated to fan operational periods to avoid large over-estimation of the PM emissions. The TEOMs provide time-stamped data required for an accurate calculation of TSP, PM10 and PM2.5 emissions.

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Table 12.2. Particulate Matter Sampling Locations and Sampling Methods/SOPs. Sidewall Fan 1 (SW1) Tunnel End (TE)

Location ID Number 1 3 Analytical Parameters TSP, PM10, PM2.5 TSP, PM10, PM2 5 Sampling SOP Appendix M, N and O Appendix M, N and O Sample Flow Rate 1 L/min 1 L/min Sampling Average Time 30 s 30 s Sampling Period Brooding Full house

12.5 Environment Conditions Sampling Electronic transmitters (Vaisala Model HMW 61U) will be used to monitor relative humidity in the houses, while type T thermocouples will be used to monitor indoor air temperature at the air sampling locations. A 0.0-0.5 inch WC (0-125 pa) differential pressure transducer (Setra Model 264) will be used to measure house static pressure. An 800-1100 mbar barometric pressure sensor (WE100) will be used to measure atmospheric pressure. For more details on the operation and specifics for the Vaisala Model HMW 61U, type T thermocouple, Setra Model 264, and WE100, see Appendix E and F. 12.6 Ventilation Rate Sampling A device for in-situ exhaust fan airflow capacity measurement, referred to as the Fan Assessment Numeration System (FANS) device, previously developed and constructed at the USDA-ARS Southern Poultry Research Laboratory, was refined and reconstructed by the University of Kentucky (Gates et al., 2004). FANS measures the total airflow rate of a ventilation fan by integrating the intake velocity field obtained from an array of five propeller anemometers used to perform a real-time traverse of the airflow entering ventilation fans of up to 122 cm (48 in) diameter. At the beginning of the project, all 14 ventilation fans in each house were calibrated by FANS and fan curves were developed. Three to four fans in each house (at least 20% of the total fans) are randomly chosen and calibrated at the beginning of each flock. The fan running status is monitored by an induction current switch (Muhlbauer et al., 2006). The voltage signal from the induction current switches attached to the fan power cords are sampled every second and recorded into the compact Fieldpoint modules every 30 seconds as the average or duty cycle of the time interval (see Appendix R). 12.7 DAQ System Recording Methods The RS232 output generated by the INNOVA 1412 analyzer, as well as the analog output signal from API 101E, VIG Model 200, TSP PM10 and PM2.5 and the analog output signal from other sensors for environmental conditions and equipment operations monitoring are logged by the National Instruments (NI) compact Fieldpoint control and measurement modules. The NI compact Fieldpoint is an expandable programmable automation controller composed of rugged I/O modules and intelligent communication interfaces. The monitoring and controlling program generated from LabView 7 is downloaded to the embedded controller and sensors for temperature, RH, and pressure are connected directly to the analog and discrete I/O modules.

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of 11 The I/O modules are the cFP-TC-120 8-Channel Thermocouple input module, the cFP-AI-110 8-Channel Analog Voltage and Current input module, the cFP-AI-112 16-Channel Analog Voltage, and the cFP-DO-400 8-Channel digital output module. The signals from the analyzers and sensors are sampled every second and recorded on the compact Fieldpoint modules and on-site PC every 30 seconds as average or duty cycle of the time interval, see Appendix G. The recorded data will be managed by the following procedures in Section 20. Specifics sheets for the above listed materials are provided in Appendix U. 12.8 Sampling/Measurement System Corrective Action Corrective action measures in the gas concentration, particulate concentration, ventilation rate, environment conditions, and DAQ system recording will be taken to ensure the data quality objectives are attained. There is the potential for many types of sampling and measurement system corrective actions. If the corrective actions involve calibration, recalibrate the instrument using the SOP for the instrument. Section 8.1 provides a list of instrument SOPs and their associated Appendix identification. Table 12.3 details expected problems and corrective actions.

Table 12.3. Possible problems and planned corrective actions. Item Problem Action Notification Gas Concentration (Routine QC check twice/week)

NH3, CO2, NMHC, or CH4 concentration from INNOVA 1412 out of Specification (± 5% of QC standard)

1. Check sampling line connection. 2. Replace inlet filter. 3. Recalibrate

Document on field data sheet

Gas Concentration (Routine QC check twice/flock)

H2S concentration out of Specification (± 5% of QC standard)

1. Check sampling line connection. 2. Recalibrate


Gas Concentration (Routine QC check twice/week)

NMHC or CH4 concentration from VIG 200 out of Specification (± 5% of QC standard)

1. Check sampling line connection. 2. Recalibrate


Gas Sampling (Routine QC check twice/week)

Low flow rate in sampling line

1. Check solenoid valve and pump. 2. Check in line filters. 3. If any valve or pump fails, replace it. 4. If inline filter is clogged, replace it.


Gas Sampling (Routine QC check once/week)

Sampling line air leakage

1. Check all tubing adaptors on the sampling line. 2. If needed, change the adaptors.


Gas Sampling (Daily QC on-line check)

Heat traced and heat taped sampling line temperature out of control

1. Turn off all pumps and stop sampling. 2. Check program. 3. Check line voltage. 4. Check control module. 5. Check control relay.

Document on field data sheet, notify ISU personnel

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Item Problem Action Notification PM Concentration (Routine QC check once/week)

Air leak Inspect all seals and O-rings, replace as necessary and re-perform leak test


Environment Conditions (Between flocks QC check)

Temperature out of Specification (±0.5°C)

Replace thermocouple Document on field data sheet

Environment Conditions (Between QC flocks)

Relative humidity out of Specification (±5% of QC standard)

Recalibrate Document on field data sheet

Environment Conditions (QC check 1/Six months)

Barometric pressure out of Specification (±5% of QC standard)


Environment Conditions (Between flocks QC check)

Static pressure out of Specification (±5% of QC standard)


Power (Daily QC on-line check)

Power Interruptions 1. Check UPS log event from computer. 2. Check line voltage

Document on field data sheet, notify field manager

DAQ (Daily QC on-line check)

PC locked up Reboot Document on field data sheet, notify ISU personnel


No internet connection

1. Check satellite modem. 2. Check satellite dish. 3. Check computer setup, open remote desktop. 4. If needed, reboot modem 5. If needed, contact with vender.



No connection between compact Fieldpoint and PC

1. Check cable. 2. Check router. 3. Check PC IP address.


Instrument (Daily QC on-line check)

Instrument failure 1. Contact ISU personnel. 2. Contact vender for technical support.


Ventilation Rate (Between flock QC check)

Current Switch failure Replace Document on field data sheet

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of 11 12.9 Litter Sampling The Iowa State University Agricultural and Biosystems Engineering Agricultural Waste Management Laboratories will conduct litter analysis for the project. This laboratory routinely conducts these analyses for use in peer-reviewed research. The litter analysis is not used in any way to determine air emissions from the facility. It is being conducted and provided in an effort to better describe the systems that are being monitored as part of this project. During litter sample collection, the sampler should wear gloves and wash their hands after handling the material. When sample compositing is necessary, composites should be mixed in a clean and dry container. Additional sample handling requirements are addressed in Section 13.2. If the sampler sees areas within the sampling zone that are irregular (i.e., a leaky waterer has created a very wet spot), this area should be sampled separately and not included in the composite. A very wet sample could interfere with the sampling results by eschewing the data. A note about the additional sample should be included on the chain of custody form. Necessary sampling equipment is described below, no additional materials or reagents are required. If procedural changes are required, they should first be approved by the project PIs. The change will then be documented in the QAPP. If a procedural change needs to take place in-situ without approval, the change should be noted in the Site Visit Report (Section 9.3) and recorded on the Chain of Custody form. Fresh and Pre-Cleanout Litter Sampling The differences between brooding areas and non-brooding areas in terms of organic matter and nitrogen content and proximity of feeders and waterers to the sampling point within a broiler house make accurate sampling and nutrient testing essential if best management practices are to be followed during handling and land application of poultry litter (Singh et al., 2004). Currently, there are two preferred methods that are suitable for sampling litter, the trench and the point methods (random walking method). In the case of very dry litter (e.g., dry matter of 80% or more), it can be very difficult to dig a trench and obtain an intact sample using a shovel. Location of water lines and feeders may further complicate the process of digging trenches. It is also difficult to sample litter using the trench method when the birds are in the house. Alternatively, litter can be sampled using the point or random walking method. For this method, the number of random sampling points within each zone of a section should be proportional to the contributing area of that zone (Figure 12.3). Both the trench and point method lead to similar results but the point method has easy implementation with representative samples for analysis. The point method (or random walking method) is used for sampling broiler litter in this study. For the point method the broiler facility is divided in two main zones: non-brooding and brooding zone. Each zone is subdivided in three sections, for replication.

Zone: division of the facility (two zones per one facility) Section: division of the zone (three sections per one zone)

The sampling points are distributed uniformly in each section. In order to obtain representative samples from each zone, the number of sub-samples taken from each section in areas affected by

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of 11 sidewall, feeders, waterers, and the central area are proportional to the areas they represented in the house. Twenty random samples are collected from each section inside of a zone, and pooled together to form one composite sample per section (three composite sub-samples per zone). Samples are collected when fresh litter is placed in the houses and prior to a full clean-out of the houses (full house clean out occurs about every 4-5 flocks, as determined by Tyson facility operators). The samples are collected with a tulip bulb digger to a maximum depth of 7.6 cm. Samples from each subsection (20) are pooled together in a container and mixed thoroughly using a shovel before collecting a composite sample. About a 1 kg sample from each subsection is stored in labeled plastic bags and transported in a cooler with ice packs to keep the temperature near 4 C. The excess sample left in the container is discarded. The sampling equipment is decontaminated by cleaning them with detergent, preferably anti-bacterial, after sampling each house. Between Flock Caked Litter Sampling During the clean up between the flock, only the surface layer of litter (referred to as “cake”) is removed from the house. Shovel samples are taken from each load of removed cake and combined to form two, 20 L samples which are stored in plastic buckets. The two buckets are labeled and transported to a freezer at the UK Research and Education Center (less than an hour of transport time). Sample Identification The sample labels include site ID, sampling zone, sampling section and date. For example, a sample collected from site 3-3, from the brooding area and from the west side of the brooding area on Feb. 3, 2006 will be labeled as 3-3 loose B1 020306 where,

Site ID: 3-3 or 1-5 Type of litter: Loose broiler litter: Loose Caked boiler litter: Cake Sampling Zone: Brood Area: B Non-Brood Area: N Section: West side: 1 Middle: 2 East side: 3 Date: mmddyr

The samples will be collected after the removal of each flock, and will be analyzed for pH, moisture content, ammonia, and total Kjeldahl nitrogen. Information on the analytical methods and quality control are provided in Section 14.

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Brooding (West) Non-brooding (East)

Sidewall area

Waterer and feeders

Central area

Waterer and FeedersSidewall area

Point Sample

N

Figure 12.2. Schematic of litter sampling scheme.

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13.0 Sample Handling and Custody 13.1 Gaseous and Particulate Matter Samples Data recorded by the monitoring equipment will be available to authorized project members through remote viewing using LabView 7 over the Internet and will be handled and recorded as described in Section 20: Data Management and in Appendix I. 13.2 Litter Samples Litter samples will be collected and prepared for transport by project team members located in Kentucky. John Earnest is responsible for overseeing sample collection and shipping. When litter samples are collected as described in Section 12.9: Litter Sampling, the following handling method is used. All collected samples are solid in nature. In-house, total litter samples are collected in one gallon air tight bags and cake litter samples are collected in 20 L plastic buckets. Samples are labeled by sample type, location, and date. An example of the sample label is included in Figure 13.1. Collected samples are transported to the UK Research and Education Center with a completed chain of custody form and stored in a freezer for transport to ISU for analysis. The chain of custody form is shown in Figure 13.2. The form is completed by the sampler and shipped with the samples in the cooler inside of a Ziplock bag to the Agricultural Waste Management Lab at ISU. After packing the cooler for transport, the cooler is closed and a chain of custody seal is placed over a location on the cooler closure. The cooler is then taped closed with clear packing tape with part of the tape covering the custody seal. The seal is a 6 in piece of masking tape with the sampler’s signature and date. Samples are either shipped within 24 hrs via a ground transportation service or brought back by individuals returning to Iowa after working at the project site. If samples are shipped, the individual initiating the shipment contacts Nurun Nahar ([email protected]) via email to notify her of the samples arrival and to provide her with a shipment tracking number. Samples are shipped to:

Nurun Nahar Iowa State University 3252 NSRIC Ames, IA 50011

Figure 13.1. Example litter sample label.

Sample Date: ______________ Sample ID: ________________ Sample Type: ______________

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Page 2 of 3 Upon arrival at the laboratory, the laboratory manager (Nurun Nahar) checks for shipment integrity and ensures the chain of custody seal is still intact on the cooler closure. The chain of custody form is retrieved from the samples. The completed chain of custody form is filed in the laboratory. Samples are then placed in the cooler until analysis (see Section 14.1). Regulatory requirements indicate samples should be analyzed for ammonia and total Kjeldahl nitrogen to be analyzed within 28 days of collection. Samples are analyzed in the Agricultural Waste Management Laboratory at ISU. Samples are analyzed for pH, moisture content, ammonia and total Kjeldahl nitrogen. Samples arriving at the Agricultural Waste Management Laboratory are logged into the laboratory’s “Samples to Analyze” notebook. Information entered into the notebook for each sample set includes: date of arrival, sample sender, sample receiver, sample storage (refrigerator, freezer, freezer to freeze dry, or ambient), sample set ID and date, required analyses, and project ID. Analyzed samples are held by the laboratory until the results are reviewed. After acceptance of the litter analysis data, the project PIs give the laboratory permission to dispose of the samples. It is the responsibility of the lead PI, Robert Burns, to oversee the filing and archiving of the sample handling documents.

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Sample Collection and Chain of Custody Form (fill out one form for each shipping container used)

Sample Collector Information

Shipping Information For Lab Use Only

Organization Name:

Address:

Lab Name: Iowa State University Agricultural Waste Management Lab Address: 3165 NSRIC Ames, IA 50010 Ph.: (515) 294-4167 Fax: (515) 294-4250

Sampler Name:

Date Shipped: Carrier:

Date received: Time received: Sample temperature on receipt: Sample condition on receipt:

Sample Identification and Collection Information Facility ID: Sample

collection point ID:

Sample collection date:

Sample volume:

Number of containers per sample:

Additional Comments:

Lab Use: Sample Seal in Place - Yes ______ No______

Sampler signature:

Date:

Lab technician signature:

Date:

Figure 13.2. Litter sample chain of custody form.

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14.0 Analytical Methods 14.1 Litter Samples All litter samples will be processed by the Agricultural Waste Management Laboratory in the Department of Agricultural and Biosystems Engineering at ISU. Upon arrival, samples are placed in the freezer -20°C in their original sampling collection containers until analysis. Moisture Content, pH, extractable ammonia and total Kjeldahl nitrogen (TKN) are analyzed. The methods, equipment, required quantity and container to be used are shown in Table 14.1. Full method descriptions and operating procedures are included in Appendix S. The laboratory manager is responsible for obtaining and completing the Chain of Custody form. The manager acts as the common point of reference between activities performed in the laboratory and activities required by the project PIs. The laboratory manager is responsible for result reporting and laboratory analysis quality control (QC) checks. If the laboratory manager needs to modify the planned laboratory activities, she will contact the PIs via email to explain the modification and request approval. The PIs will discuss the modification and approve or disapprove as necessary. The laboratory currently maintains QC by performing triplicate analysis on methods for moisture content, pH, ammonia, and TKN; and spike matrices on methods for ammonia and TKN. Triplicate analyses and spiked matrices are performed on one sample for each set of samples analyzed. Blanks, or high purity water, are a part of the methods for pH, ammonia, and TKN as described in Appendix S. The spike is performed at a concentration 1.5 times the expected level of the sample (expected sample concentration will vary dependent on litter age and location within the house). Analyzed samples are placed in a freezer at -20°C for archiving until the project PIs permit sample disposal. Samples will be disposed of in accordance with ISU Environmental Health and Safety requirements. If a failure in one of the analytical systems occurs, Lara Moody is to be contacted. She will then notify the lead project personnel. If the problem cannot be resolved in a time period sufficient to complete the analyses, the samples will be analyzed using an equivalent alternative method or instrument.

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Table 14.1. Methods for litter analysis.

Parameter Method Quantity Container* Preservative Analytical Instrument

pH (water 1:2)

Manure pH (Combs et al., 2003) 20 g

Ziplock bag or plastic bucket

Cool to <4°C Orion 4-Star pH meter

Moisture Content

Standard Method 2540 G

(APHA et al., 1998) 2 g


Cool to <4°C Fisher Isotemp Oven

Ammonia Standard Methods 4500-NH3 B & C

(APHA et al., 1998) 20 g


Cool to <4°C Labconco Rapid Still II

Total Kjeldahl Nitrogen

Standard Methods 4500-Norg

D and C (APHA et al., 1998)

5 g Ziplock bag

or plastic bucket

Cool to <4°C

Labconco Block Digester

and Rapid Still II

* See sample method description and sample handling in Sections 12.9 and 13.2.

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15.0 Quality Control Measures Quality assurance and quality control include the use of properly maintained and reliable instrumentation, approved analytical methodologies and standard operating procedures, external validation of data, well-trained analysts, audits, and documentation. When appropriate, published EPA analytical methodologies are used. The QC measurements for all instruments are listed in Table 15.1. Logs are maintained for each instrument. Reports are generated after each QC measurement. Specific quality control procedures will include the following:

1. A measurement of certified zero air is included as a field blank for gas concentration measurements once a week.

2. A replicated multipoint calibration of analyzers is performed initially and whenever the span checks are beyond the acceptable limits shown in Table 15.1.

3. Calibration checks (zero and span) of gas analyzers are conducted twice a week by introducing the calibration gas into the gas sampling collecting manifold M2 (see Appendix B). Calibration records are maintained in the project logbook.

4. Thermocouples are calibrated before and after the 6-month collection period with spot checks of each sensor every flock.

5. Relative humidity probes are tested with a National Institute of Standards and Technology (NIST) transfer standard or equivalent every 6 months.

6. Calibrations of the differential pressure transmitters are conducted every 6 months. Zero checks are conducted every flock.

7. Barometric sensors are tested every 6 months and calibrated if the zero or span drift is beyond the acceptable limit shown in Table 15.1.

8. The TSP, PM10 and PM2.5 TEOM analyzers are maintained weekly and calibrated yearly. 9. Online results of all the continuous measurement variables are displayed on a PC video

monitor and published to the Web where continuous Internet connection is available. Project personnel check the online display at least daily by either remote or on-site access.

10. An email alarm mechanism was developed and is used when critical data is out of range, which could be caused by malfunction of instruments, over detection limit of instruments and power failures. The alarm email is generated automatically by the program and sent to all project personnel. The problems are addressed and solved the next business day.

11. Data files logged in the PC on the previous day are checked the next business day to find and correct any problems with the system.

12. Experienced analysts run all equipment. 13. An uninterruptible power supply with battery backup is used to prevent damage to sensitive

equipment and data loss in case of power failure. 14. Surge suppressors are used to protect the PC and the instruments. 15. Internal performance and internal and external system audits are performed to evaluate the

accuracy of field measurements of air pollutants.

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Page 2 of 14 Table 15.1 is categorized by the type of QC check as listed below. All QC measurements are documented and reports are generated to record all activities. Further descriptions of these checks are provided in Section 15.1, 15.2 and 15.3.

1. Calibration standard quality control check. The QC check is done in the Lab, and the vendor will provide the certificate for all calibration gas.

2. Calibration/Verification field check. The instruments are calibrated or verified, and the vendor will provide the certificate for all calibration gas.

3. Field accuracy and bias QC check. The check is performed regularly twice per week or between flocks

4. Data quality check audit. Data review and processing.

The concentrations of the NIST traceable calibration gases used are shown in Table 15.1. There is no NIST traceable NH3 calibration gas available. Certified Plus Grade NH3 calibration gas with ± 2% accuracy against manufactory standard will be used as standard for INNOVA 1412 analyzer. Selection of the gas concentration is dependent on the normal range for each pollutant. Information about the calibration gases is shown below.

Calibration Gas Accuracy Standard

N2 zero gas 99.999% purity 99.999% purity

Certified Plus Grade NH3 mixture balanced in air/nitrogen ±2% accuracy

25 ppm manufactory

standard EPA Protocol mixture CO2 balanced in nitrogen ±1% accuracy 2000ppm NIST

traceable EPA Protocol mixture CH4 balanced in nitrogen ±1% accuracy 3 or 80 ppm NIST

traceable EPA Protocol mixture propane balanced in nitrogen ±1% accuracy 3 ppm NIST

traceable EPA Protocol mixture H2S balanced in nitrogen ±1% accuracy 10.7 ppm NIST

traceable In field QC checks, the NIST-traceable cal-gases are used for INNOVA 1412, API 101E and VIG 200; transfer standards are used for thermocouple, static pressure sensor, flow meter, relative humidity and barometric sensor.

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Table 15.1 QC checks of the project. QC

Check Requirement Instrument Fre-

quency Acceptance Criteria Standard Reference Information

provided Flow rate (transfer standard)

Mass Flow meters 1/yr ±2% of NIST-

traceable standard

1 LPM, 15.67 LPM, 16.67

LPM

Certification of Traceability

Thermometer (transfer standard)

Thermometer 1/yr ±0.1°C resolution ±0.5°C accuracy Full scale Certification of

Traceability

Barometer (transfer standard)

Barometer 1/yr ±1 mm Hg

resolution ±5 mm Hg accuracy

Fortin Barometer Certification of

Traceability

Static presser (transfer standard)

Static Presser sensor

1/yr ±1.25 Pa accuracy Full scale Certification of Traceability

N2 zero gas Gas bottle Every

new gas tank

99.999% Purity 99.999% Purity Provided by vendor


25 ppm certified plus grade NH3

mixture balanced in

air/N2

Gas bottle Every

new gas tank

±2% accuracy Manufactory standard

Provided by vendor


2000 ppm EPA Protocol

mixture CO2 balanced in N2

Gas bottle Every

new gas tank

±1% accuracy NIST traceable standard

Provided by vendor


80 ppm EPA Protocol

mixture CH4 balanced in N2

Gas bottle Every

new gas tank


Provided by vendor


3 ppm EPA Protocol mixture propane

balanced in N2

Gas bottle Every

new gas tank


Provided by vendor


100-1000 ppb EPA Protocol mixture H2S

balanced in N2

Gas bottle Every

new gas tank


Provided by vendor


3 ppm EPA Protocol mixture propane

balanced in N2

Gas bottle Every

new gas tank


Provided by vendor


Cal

ibra

tion

Stan

dard

(Lab

QC

)

3 or 80 ppm EPA Protocol mixture CH4

balanced in N2

Gas bottle Every

new gas tank


Provided by vendor


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Zero point Innova 1412

API 101E VIG 200

If accuracy

check failed

±5% of Standard gas N2 zero gas

Appendix D, K and

L

Calibration drift/

Verification to assure proper

function

NH3 optical filter Innova 1412

If accuracy

check failed

±5% of Standard gas (25ppm)

25 ppm manufactory

traceable NH3 balanced in air/

N2

Appendix D

Calibration drift/


function

CO2 optical filter Innova 1412

If accuracy

check failed


2000 ppm NIST traceable CO2 balanced in N2

Appendix D

Calibration drift/


function

CH4 optical filter Innova 1412

If accuracy

check failed

±5% of Standard gas (80 ppm)

80 ppm NIST traceable CH4 balanced in N2

Appendix D

Calibration drift/


function

Non-CH4 optical filter Innova 1412

If accuracy

check failed


3 ppm NIST traceable propane

balanced in N2

Appendix D

Calibration drift/


function

H2S optical filter API 101E

If accuracy

check failed

±5% of Standard gas (100-1000 ppb)

100-1000 ppb NIST traceable H2S balanced

in N2

Appendix K

Calibration drift/


function

NMHC optical filter VIG 200

If accuracy

check failed


3 ppm NIST traceable propane

balanced in N2

Appendix L

Calibration drift/


function

CH4 optical filter VIG 200

If accuracy

check failed

±5% of Standard gas (3 or 80 ppm)

3 or 80 ppm NIST traceable CH4 balanced

in N2

Appendix L

Calibration drift/


function

Cal

ibra

tion/

Verif

icatio

n (F

ield

QC

)

Temperature sensor

Type-T Thermocouple

If accuracy

check failed

±0.5°C Transfer standard

Appendix E

Calibration drift/


function

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Static pressure sensor

Setra 264

If accuracy

check failed

±5% of full scale (124.5 Pa)

Transfer standard

Appendix F

Calibration drift/


function

Relative humidity sensor

Vaisala HMW61U

If accuracy

check failed

±5% 33% and 75% Appendix E

Calibration drift/


function

Barometric pressure WE100

If accuracy

check failed

±5% of Full scale (101325 Pa)

Transfer standard

Appendix P

Calibration drift/


function

Flow controller (software) TEOM

If accuracy

check failed

±5% of Standard (1 or 15.67 LPM)

Transfer standard

Appendix M, N, O

Calibration drift/


function

Flow controller (hardware) TEOM

If accuracy

check failed

±5% of Standard (1 or 15.67 LPM)

Transfer standard

Appendix M, N, O

Calibration drift/


function

Analog I/O Amplifier

board Ambient air

temp Ambient pressure

Mass transducer

TEOM 1/yr ±5% of Transfer standard

Transfer standard

Appendix M, N, O

Calibration drift/


function

GSS leak check GSS 1/week <0.1 LPM Transfer

standard Appendix

B Measure

system bias

GSS flow rate check GSS 2/week >7 LPM Transfer

standard Appendix

B

Measure system bias /Pump flow rate bias

Zero point Innova 1412 VIG 200 2/wk ±5% of Standard

gas N2 zero gas Appendix D, K, L

Instrument bias

NH3 Innova 1412 2/wk ±5% of Standard gas (25ppm)

25 ppm manufactory

traceable NH3 balanced in

air/ N2

Appendix D

Instrument bias

Accu

racy

or B

ias

(Fie

ld Q

C)

CO2 Innova 1412 2/wk ±5% of Standard gas (2000ppm)

2000 ppm NIST traceable CO2 balanced in N2

Appendix D

Instrument bias

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CH4 Innova 1412 2/wk ±5% of Standard gas (80 ppm)

80 ppm NIST traceable CH4 balanced in N2

Appendix D

Instrument bias

Non-CH4 Innova 1412 2/wk ±5% of Standard gas (3ppm)

3 ppm NIST traceable Propane

balanced in N2

Appendix D

Instrument bias

H2S API 101E 2/flock ±5% of Standard gas (100-1000 ppb)

100-1000 ppb NIST traceable H2S balanced

in N2

Appendix K

Instrument bias

NMHC VIG 200 2/wk ±5% of Standard gas (3ppm)

3 ppm NIST traceable Propane

balanced in N2

Appendix L

Instrument bias

CH4 VIG 200 2/wk ±5% of Standard gas (3 or 80 ppm)

3 or 80 ppm NIST traceable CH4 balanced

in N2

Appendix L

Instrument bias

Static pressure (0 point)

Setra 264 1/Flock ±5% of Transfer standard

Transfer standard

Appendix F

Instrument bias

Relative humidity

Vaisala HMW61U

1/Six months ±5% 33% and 75% Appendix

E Instrument

bias Barometric pressure WE100 1/Six

months±5% of Transfer

standard Transfer standard

Appendix P

Instrument bias

Leak check TEOM 2/Flock Main flow≤0.15 LPM Aux flow≤0.65 LPM

Internal controller

Appendix M, N, O

Instrument bias

Exhaust fan FANS 1/flock ±10% Previous check Appendix C

Instrument bias

System check All instruments Daily normal operation

range Appendix I

Data processing

Raw data check

DAQ system Daily completeness >75% Appendix

I Data

processing

Dat

a Q

uality

(Lab

Q

C)

Processing data

DAQ system Daily completeness >75% Appendix

I Data

processing

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Page 7 of 14 15.1 Calibration Calibration is the comparison of a measurement standard or instrument with another standard or instrument to report, or eliminate by adjustment, any variation (deviation) in the accuracy of the item being compared. The purpose of calibration is to minimize bias. For air and PM, calibration activities follow a two step process:

1. Certifying the calibration standard and/or transfer standard against an authoritative standard 2. Comparing the calibration standard and/or transfer standard against the routine

sampling/analytical instruments Calibration requirements for the critical field and equipment are found in Table 15.1; the details of the calibration methods are included in the calibration section (Section 17) and Appendixes for SOPs. 15.2 Accuracy or Bias Checks Accuracy is defined as the degree of agreement between an observed value and an accepted reference value and includes a combination of random error (precision) and systematic error (bias). In this program, the following accuracy checks are implemented: • GSS leak check and flow rate checks • Gas analyzer checks • TEOMs flow rate audit • TEOMs leak checks • Static pressure checks • Relative humidity checks • Barometric pressure checks • Exhaust fans flow rate checks

GSS Leak Check and Flow Rate Check The response times of the analyzers have been tested in the lab. However, the actual on-site performance of the sampling system had to be tested also. Therefore, ammonia span gas was injected into a sampling line on-site through the longest sampling line (tunnel end) (Figure 15.1). The results of INNOVA 1412 analyzers from both houses are shown in Figures 15.2 and 15.3. For both sampling system, the fourth ammonia concentration readings (30 s × 4 = 120 s) reached 96% and 97% of the span concentration.

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Figure 15.1. Picture of span gas injection from sampling points.

INNOVA 1412

Tyson 1-5_Tunnel

0

65

83

22

1512

9 10 10 8

100 100 1011009897 9997

94

0

20

40

60

80

100

0:00 0:30 1:00 1:30 2:00 2:30 3:00 3:30 4:00 4:30 5 00 5:30 6:00 6:30 7:00

Time,min:sec

Perc

enta

ge,%

0

5

10

15

20

25

NH 3

Con

cent

ratio

n, p

pm

Figure 15.2. Tyson 1-5, sampling system and INNOVA analyzer response time check.

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INNOVA 1412Tyson 3-3_Tunnel

0

75

89

94

100999997

10096

0

20

40

60

80

100

0:00 0:30 1:00 1:30 2:00 2:30 3:00 3:30 4:00 4:30 5:00 5:30Time, min:sec

Perc

enta

ge,%

0

5

10

15

20

25

NH 3

Con

cent

ratio

n, p

pm

Figure 15.3. Tyson 3-3, sampling system and INNOVA analyzer response time check.

As well as using span gas to challenge the sampling system at one location, multiple point sampling system tests have been done by comparing the readings of INNOVA 1412 analyzer inside of the monitoring trailer with 3 INNOVA 1412 analyzers located at three sampling locations (SW1, SW3 and TE). Three INNOVA 1412 analyzers were located near the three sampling locations and continuously took samples during the whole testing period (Figure 15.4). All INNOVA 1412 analyzers were synchronized and calibrated by the same NH3 calibration gases before this test.

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Figure 15.4. INNOVA side-by-side comparison between in-house and MAEMU NH3 readings.

At Tyson 1-5 site, the number of sampling cycles per location of the INNOVA in the MAEMU was set to 4, 6 and 8 per location for testing the response time effect. The NH3 readings from the INNOVA 1412 in the MAEMU were compared with the readings in three locations (Figure 15.5). Only the last readings from the MAEMU in each sampling cycle at each location were compared with the most recent readings from the INNOVAs in the houses. At the Tyson 1-5 site, five pairs of readings for each sampling number at each location were chosen. The two-way ANOVA test was used for the statistical analysis. There was neither a sampling number effect nor location effect (P = 0.37). Table 15.2 provides a comparison of continuous in-house NH3 readings with those obtained from location cycling by the MAEMU INNOVA at 4, 6, or 8 sampling iterations from Tyson 1-5 (unit: ppm). It indicated that the NH3 reading in the MAEMU matched the reading in the house at all three locations and there was no difference for using 4, 6 and 8 sampling numbers at each location. As such, four sampling iterations were chosen to reduce the time required to cycle from each sampling location in the house. Because fan operation periods can be as short as 30 seconds in a typical broiler facility, it is very important to move between sample locations quickly to capture temporal variability because of fan operation cycles as ammonia-laden air is exhausted and fresh air is introduced through the box inlets. Because four samples were proven to provide equivalent performance as a higher sampling frequency, only a 4-cycle test was performed at Tyson 3-3. The value of this test at both Tyson 1-5 and Tyson 3-3 was to provide an indirect leak check of each sample line system and the GSS in each MAEMU. Since the NH3 reading in the MAEMU matched the reading in the house at each location, it can be concluded that no dilution air was entering the system, thus, no leakage was occurring.

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Comparison and Sample Frequency Test at Tyson 15, Feb 8 2006

0

5

10

15

20

25

30

13:12 13:40 14:09 14:38 15:07 15:36 16:04

Time, hr:min

Am

mon

ia C

once

ntra

tion,

ppm

NH3_sw1_TrailerNH3_sw3_TrailerNH3_T_TrailerNH3-sw1NH3-sw3NH3-Tunnel4 samples per location

8 samples per location

6 samples per location

Figure 15.5. Ammonia readings from the MAEMU and in-house INNOVAs.

At Tyson 3-3, six pairs of readings at each location with four sampling numbers were chosen. A one-way ANOVA test was used for the statistical analysis. There was no location effect for NH3 reading in the trailer (P = 0.26). Table 15.3 provides a comparison of continuous in-house ammonia readings with those obtained from location cycling by the MAEMU INNOVA at four sampling iterations at Tyson 3-3 (unit: ppm). The mean values are NH3(in-house) – NH3(MAEMU).

It indicated that the NH3 reading in the trailer matched the reading in the house at all three locations.

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Page 12 of 14 Table 15.2. Comparison of in-house NH3 readings with those obtained from

location cycling by the MAEMU INNOVA. NH3(in-house) – NH3(MAEMU)

For sampling locations of P = 0.37 No. of Sampling Iterations SW1 SW3 Tunnel

Mean (ppm) SD

4 0.72 0.20 0.31 0.41a 0.65 6 0.26 0.08 -0.19 0.05a 0.37 8 0.18 -0.02 0.46 0.20a 0.39 Mean 0.39 b 0.09 b 0.19 b Total mean 0.22 SD 0.66 0.33 0.40 Total SD 0.50 *Column or row means with the same superscript letter are not significantly different (P > 0.10).

Location Mean (ppm) SD

SW1 0.45 a 0.46 SW3 0.03 a 0.83 Tunnel -0.27 a 0.98 Total 0.03 0.82 *Column means with the same superscript letter are not significantly different (P > 0.10).

Flow meter 1

Flow meter 2

Pump

GSS Board Sampling tubing

Figure 15.6. Gas sampling line leak check.

Sampling Line Check During weekly field visits, each sampling line is checked by adding an additional flow meter at the pump-end and blocking the sampling port in-house (Figure 15.6). If the additional flow meter reads zero, it indicates there are no leakages in the sampling line with negative pressure.

Corrective action—The whole sampling line and all connectors will be inspected and the leakage will be sealed.

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Page 13 of 14 GSS Flow Rate Check The sampling flow rate at each sampling line is checked by monitoring the air flow rate at each sampling port through an in-line flow indicator. The flow rate change between two check points should be lower than the QC standard.

Corrective action—The whole sampling line and all connectors will be inspected and the leakage will be sealed. If no leakage developed in the sampling line, the sampling pump will be rebuilt.

Gas Analyzer Checks The analyzers of INNOVA 1412, API 101E and VIG 200 are challenged by NIST-traceable calibration gases. The interferences of each gas are tested as well. For INNOVA 1412, the interference of gases will be compensated by the analyzer self. For API 101E and VIG 200, the interference will be recorded.

Corrective action—The analyzer will be calibrated.

TEOMs Flow Rate Audit This flow rate audit corresponds to the flow controller audits. Details of the audit are included in the TEOM manual and Appendixes M, N and O. The audit is made by measuring the analyzer’s normal operating flow rate using a certified flow rate transfer standard.

Corrective action—The flow controller will be calibrated.

TEOMs Leak Checks A leak check is performed after every time the location of the TEOMs is changed and when the inlet is changed. A leak test kit will be used.

Corrective action—The whole sampling lines and all connectors will be inspected and the leakage will be sealed.

Static Pressure Checks The static pressure sensors are tested under “0” differential pressure condition. Details of the audit are included in the SOP of differential static pressure sensor transmitters (Appendix F).

Corrective action—The transmitter will be calibrated.

Relative Humidity Checks The relative humidity sensors are tested with multiple points. Details of the audit are included in the SOP of temperature and humidity measurement (Appendix E).

Corrective action—The transmitter will be calibrated. Barometric Pressure Checks Details of the audit are included in Appendix P. The audit is made by measuring the sensor’s normal operating pressure using a certified barometric pressure transfer standard.

Corrective action—The barometer will be calibrated.

Exhaust Fans Flow Rate Checks Twenty percent of the total exhaust fans are calibrated and details of the checks are included in Appendix C. The audit is made by measuring the fan flow rate using the FANS system.

Corrective action—All exhaust fan will be calibrated.

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Page 14 of 14 15.3 Data Quality Control Online results of all the continuous measurement variables are displayed on a PC video monitor and published to the Web; a continuous Internet connection is available. Project personnel check the online display at least daily by either remote or on-site access. An email alarm mechanism was developed and is used when critical data is out of range; out of range data could be caused by malfunction of instruments, over-detection limit of instruments and power failures. The alarm email is generated automatically by the program and sent to all project personnel. The problems are addressed and solved the next business day. Data files logged the previous day in the PC are checked the next business day to find and correct any problems with the system. Details of data processing are included in Sections 20 and 24. 15.4 Control Charts Control charts are used extensively by the project. They provide a graphical means of determining whether various phases of the measurement process are in statistical control. The project utilizes charts which graph single measurements of a standard or a mean of several measurements. Table 15.3 indicates which QC samples are control charted.

Table 15.3. Control charts. QC Check Plotting technique GSS Leak Check Single values plotted GSS Flow Rate Check Single values plotted Innova Check Single values plotted API 101E Check Single values plotted VIG 200 Check Single values plotted TEOM Leak Check Single values plotted TEOM Flow Controller Check Single values plotted Static Pressure Sensor Check Single values plotted Relative Humidity Check Single values plotted Barometric Pressure Check Single values plotted Exhaust Fans Flow Check Multiple values plotted

15.5 Litter Sampling Quality Control Checks During full house litter sampling that occurs just before litter is fully removed from the houses for a clean-out, two samples will be selected as quality control samples. These two samples will be randomly selected. The selected samples will be split into three sub-samples and delivered with the other samples to the Agricultural Waste Management Laboratory at Iowa State University for analysis. The sampler will contact Lara Moody, the QA Manager to provide the sample IDs of the split samples. Lara Moody will review the laboratory results. If corrective actions are necessary, Lara will provide a corrective action report to the PIs.

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16.0 Instrument/Equipment Testing, Inspection, and Maintenance The purpose of this element in the QAPP is to discuss the procedures used to verify that all instruments and equipments are maintained in sound operating condition and are capable of operating at acceptable performance levels. See Section 9 for document and record details. 16.1 Testing All instruments and equipment are or will be purchased new with NIST-traceable or manufactory certifications. The INNOVA 1412, API 101E and VIG 200 are calibrated with manufactory certifications. The project personnel run the analyzers at the laboratory. NIST-traceable calibration gases, when available, are used for the verification checks. Information on the calibration gases used is provided in Section 15. If any of these checks are out of specification (see Table 15.1), the project personnel contacts the vendor for initial corrective actions. Once installed at the sites, the field operators run the tests mentioned above. These tests are properly documented and filed as indicated in Section 9. 16.2 Inspection Inspection of various equipment and components are provided here. Inspections are subdivided into two sections: one pertaining to online monitoring and one associated with field activities. Online Monitoring Online monitoring is performed daily through real-time display on computers. There are several items that need daily inspection in the online monitoring. Table 16.1 details the items to inspect and how to appropriately document the inspection. Inspection of Field Items There are several items that need inspection in the field. Table 16.2 details the items to inspect in the field and how to appropriately document the inspection.

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Table 16.1. Inspections online.

Item Inspection Frequency

Inspection Parameter

Action If Item Fails Inspection

Documentation Requirement

Innova 1412

Daily Sampling frequency 30~32 sec

Check analyzer Call service provider that holds maintenance agreement

1. Document in logbook 2. Notify field personnel

API 101E Daily H2S concentration > 0 ppb



VIG 200 Daily Concentration > 0 ppm



Computer Daily Remote desktop

Reboot computer 1. Document in logbook 2. Notify field personnel

Internet service

Daily IP address Check satellite receiver and modem Call service provider that holds maintenance agreement


Heat trace temperature

Daily Temp. > 45°C Check compact Fieldpoint Check breaker Check AC relay


Heat tape temperature

Daily Temp. > 40°C Check compact Fieldpoint Check breaker Check AC relay


Static pressure

Daily ΔP > 0 when fans are on

Check compact Fieldpoint Check fuses on board Check signal wire


Trailer temperature

Daily 20-30°C Check thermostat Check heater Check AC


TEOM filter load

Daily < 10% Change filters 1. Document in logbook 2. Notify field personnel

TEOM main flow rate

Daily 1 L/min Check pump Check in-line filter Leak check


Barometric pressure check

Daily 0.97-1.0 bar Check compact Fieldpoint Check fuses on board Check signal wire


Relative humidity sensor

Daily 10-99% Check compact Fieldpoint Check fuses on board Check signal wire


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Table 16.2. Inspections performed in the field before and after samples are taken.

Item Inspection Frequency

Inspection Parameter

Action if Item Fails Inspection

Documentation Requirement

Innova 1412 Twice/wk Self check warning message


Document in logbook

API 101E Twice/wk Warning message


Document in logbook

VIG 200 Twice/wk Pressure Check analyzer Check corresponding gas tank Call service provider that holds maintenance agreement

Document in logbook

Gas tanks Twice/wk Pressure > 400psi

Replace Document in logbook

GSS flow meter

Twice/wk ~15 LPM Check pump Check connectors Check sampling tubing

Document in logbook

TEOM in-line filters

Twice/wk Loaded particulate

Change filters Document in logbook

TEOM inlet heads

Twice/wk Loaded particulate

Change inlet Document in logbook

Fuses Twice/wk Continuity Replace Document in logbook UPS Twice/wk Warning light Check software

Check breaker Document in logbook

Air compressor Twice/wk 55 psi Check pump Document in logbook Zero air generator

Twice/wk Pressure 30 PSI

Adjust regulator Document in logbook

Current switch Every flock On/Off Replace Document in logbook Power supplies Every flock Measure the

output voltage Check fuses Replace

Document in logbook

Thermocouples Every flock 0 to 50°C Replace Document in logbook Solenoid valve Every flock On/Off Replace Document in logbook TEOM pump Six months Flow drop <

90%- with kits Rebuild pump Document in logbook

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16.3 Maintenance All analytical equipment is properly tested (as described in Section 15.1) and maintained regularly to ensure it is functioning properly in accordance with the manufacturer’s recommended intervals and acceptance parameters. All equipment, including sampling pumps and analytical instruments, is inspected regularly during weekly site visits by the project field personnel. Equipment is repaired as soon as possible upon discovery of a problem. The manufacturer’s instructions for routine maintenance of equipment are followed. Standard operating procedures for each instrument included in the project are listed in the Appendices. Table 16.3 details the appropriate maintenance checks and frequency of the equipment. All testing, inspection and maintenance activities are documented in the field project logbook. An example of the logbook entry forms and entries are included in Appendix T.

Table 16.3 Preventive maintenance of field items.

Item

Maintenance Frequency Location Maintenance

Performed

INNOVA calibration Twice/week Field VIG calibration Twice/week Field TEOM inlet heads Twice/week Field TEOM filter Weekly Field Poultry scale system RSC-2 Weekly Field Computer virus check Weekly Field Sampling port filter Weekly Field Computer files backup Weekly Field TEOM leak check Twice/flock Field Polytron I Every flock Field Thermocouple Every flock Field Current switch Every flock Field Fan Every flock Field GSS sampling line Every flock Field Pump Every flock Field Solenoid valve Every flock Field Static pressure sensor Every flock Field Humidity sensor Every flock Field Barometric sensor Every flock Field Air compressor Every flock Field HVAC Every flock Field Zero air generator Yearly Field TEOM Yearly Field

At the end of each grow-out and prior to entry of the next flock, the following maintenance checklist (see Appendix T) is performed on the broiler houses. Another checklist for annual and semi-annual maintenance is shown in Appendix T.

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17.0 Instrument/Equipment Calibration and Frequency The TSP, PM10 and PM2.5 analyzers (TEOM 1400, R & P Thermo Electron, East Greenbush, NY) are maintained weekly or more often as warranted. The TEOM 1400s are calibrated yearly. See Appendix M, N and O for SOPs. TEOM filters are changed weekly and TEOM inlet heads and 2.5 micron cut cyclones are exchanged with clean units semi-weekly. At the beginning of the project, all fans were calibrated by FANS unit and fan curves were developed. Afterward, three to four fans from each house (less than 20% of the total fans) were randomly chosen and calibrated at the beginning of each flock. If the fan flow rates differences with the pervious calibration are larger than 10%, all fans were recalibrated. See Appendix C for SOP. Calibration records of gas analyzers, RH sensors, pressure transmitters and TEOMs are maintained weekly with the schedule specified by the manufacturer in accordance with applicable standard operating procedures. The maintenance and calibration of the instruments are recorded in the Maintenance/Calibration sheets developed in each SOP. The records are submitted to and maintained by ISU and UK personnel on a weekly basis. All the critical spare parts for the instruments are prepared and kept in the on-site MAEMUs. An inventory list of all spare parts is provided for each site. The manufacturer contact information is provided in the SOPs. 17.1 Instrumentation Requiring Calibration INNOVA 1412 Multi-Gas Analyzer Initially, multipoint calibration of the analyzers is conducted in triplicate. For calibration, either precision gas mixing or a dynamic dilution system is used with a span gas and zero air or with multiple cylinders of calibration gases that provide a series of concentrations spanning the range of expected analysis concentrations. Accuracy and precision of the analyzer are determined from these measurements. API 101E H2S Analyzer Initially, multipoint calibration of the analyzers is conducted in triplicate. For calibration, either precision gas mixing or a dynamic dilution system is used with a span gas and zero air or with multiple cylinders of calibration gases that provide a series of concentrations spanning the range of expected analysis concentrations. Accuracy and precision of the analyzer are determined from these measurements. VIG 200 Non-Methane Hydrocarbons Analyzer The VIG 200 non-methane hydrocarbon analyzer is challenged with zero air, an EPA protocol CH4 span gas, and an EPA protocol propane span gas. The routine check is conducted semi-weekly and the calibration is conducted if it cannot meet the QC limit of ±5%. See Appendix L for SOP.

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Page 2 of 6 Temperature, Pressure and Relative Humidity Sensors Precision ASTM mercury-in-glass thermometers (-8 to 32°C and 25 to 55°C, 0.1°C precision) are used for calibrating thermocouples in the field. A stationary mercury manometer in the UK laboratory is used as a primary standard to calibrate the electronic barometer that goes in the field. An inclined manometer is used as a standard to calibrate the differential pressure sensor. The barometric pressure transmitters (WE100, Global Water, Gold River, CA) are calibrated prior to use and recalibrated every six months. See Appendix P for SOP. The differential pressure transmitters (Model 264, Setra, Boxborough, MA) are calibrated prior to use and recalibrated at the conclusion of the test at 0 Pa and 20-40 Pa (typical building static pressure ) by direct comparison with an inclined manometer every six months. The zero is checked monthly. See Appendix F for SOP. A salt calibrator kit (Model HMK15, Vaisala, Woburn, MA) or equivalent methods are used to calibrate the capacitance-type RH sensors (HMW 61U, Vaisala, Woburn, MA) prior to commencing the study, and every six months thereafter if it cannot meet the QC limit of 5%. See Appendix E for SOP. TEOM 1400 TSP, PM10 and PM2.5 Particulate Monitors Since the TEOM monitors can be directly mass calibrated, it can be directly quality assured using a mass standard. All QA procedures are coordinated with routine maintenance procedures to minimize down time. Procedures are based on routine flow auditing, leak checking, and mass calibration verification. See Appendix M, N and O for SOPs. Field As indicated above, the following calibrations are performed in the field: • Calibration of gas analyzers in MAEMU against the bottle calibration standard gas. • Calibration of thermocouples and pressure sensors against the NIST-traceable standard or

transfer standard. • Calibration of TEOMs against pre-weighed filters certified by the manufactory. • Calibration of TEOM flow controller against a calibrated flow meter, transfer standard.

17.2 Calibration Method That Will Be Used for Each Instrument INNOVA 1412 Gas Concentration Calibration The calibration and QC checks of the INNOVA 1412 are addressed in Section 17.1 and Section 15 and Appendix D of this QAPP. The linearity of the INNOVA 1412 was tested in the laboratory before it was taken to the field. The linearity checks for INNOVA were performed at concentration ranges between 0-300 ppm, 0-4000 ppm, 0-1000ppm, 0- 3 ppm, and 0-10 ppm for NH3, CO2, CH4, propane and N2O, respectively. These concentrations are well above the maximum concentrations expected in the broiler houses. The gas concentration selected for the

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Page 3 of 6 calibration span checks is 80% of the expected concentration levels. Routine calibration checks are conducted twice per week by introducing a span gas into manifold M2 (see Figure 1 of Appendix B). In this way, the calibration gas flows through the same plumbing that the samples flow through in the trailer except for the solenoids. Every site visit, zero gas and span gases are manually introduced into the analyzer. For INNOVA 1412 analyzers, PC-based calibration software (Gas Monitoring Software 7304, INNOVA) will allow consistent calibration, thus eliminating human error. The INNOVA 1412 analyzers are challenged with zero air, span calibration gases. Certifications for calibration gases are according to EPA protocol, where available for a given concentration. The certified calibration gases consist of zero air, NH3 in N2, CO2 in N2, Methane in N2 and Propane in N2. All calibration gases need to have a certificate of analysis and not be used outside their expiration date. When calibration gases expire, new cylinders are purchased. API 101E H2S Gas Concentration Calibration The calibration and QC checks of the API 101E are addressed in Section 17.1 and Section 15 and Appendix K of this QAPP. The linearity of the API 101E was tested in the lab before the instrument was taken to the field. The range of linearity check for API was 0-1000 ppb, extending well above the concentrations expected in the broiler house. The gas concentration selected for the calibration span checks was 90% of the expected concentration levels. Routine calibration checks are conducted twice per week by introducing a span gas into manifold M2 (see Figure 1 of Appendix B). In this way, the calibration gas flows through the same plumbing that the samples flow through in the MAEMU except for the solenoids. Every week, zero gas and diluted span gas are manually introduced into the analyzer. Certifications for calibration gases are according to EPA protocol, where available for a given concentration. The certified calibration gases consist of zero air, H2S in N2. All calibration gases need to have a certificate of analysis and cannot be used outside their expiration date. When calibration gases expire, new cylinders are purchased. VIG 200 Gas Concentration Calibration The calibration and QC checks of the VIG 200 are addressed in Section 17.1 and Section 15 and Appendix L of this QAPP. The VIG 200 non-methane hydrocarbon analyzer is challenged with zero air, an EPA protocol methane span gas and an EPA protocol propane span gas. The routine check is conducted semi-weekly and the calibration is conducted if it cannot meet the QC limit of ±5%. See Appendix L for SOP. All calibration gases need to have a certificate of analysis and cannot be used outside their expiration date. When calibration gases expire, new cylinders are purchased. Thermocouple Temperature Calibration Procedure All thermocouples for sampling ports are calibrated once per flock. A three-point verification/calibration is conducted at the field site. Several steps to follow in calibrating ambient air temperature are given in the following summary: • Remove the ambient temperature thermocouple from the sampling pipe. Prepare a

convenient container (an insulated vacuum/wide mouth thermos bottle) for the ambient temperature water bath and the ice slurry bath. Wrap the sensor(s) and a thermometer

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Page 4 of 6 together with rubber band; ensure that all the probes are at the same level. Prepare the ambient or ice slurry solution. Immerse the sensor(s) and the attached thermometer in the ambient temperature bath. Wait at least 5 minutes for the ambient thermal mass and the sensor/thermometer to equilibrate. Wait at least 15 minutes for equilibration with the ice slurry before taking comparative readings.

• For each thermal mass, in the order of Ambient, Cold, Ambient, Hot, Ambient, make a series of five measurements, taken about 1 minute apart. If the measurements indicate equilibrium, average the five readings and record the result as the sensor temperature relative to the thermometer.

Pressure Calibration Procedure A barometer can be calibrated by comparing it with a secondary standard traceable to a NIST primary standard. Protect all barometers from violent mechanical shock and sudden changes in pressure. A barometer subjected to either of these events must be recalibrated. Locate the instrument so as to avoid direct sunlight, drafts, and vibration. A Fortin, mercury type barometer, is used in the laboratory to calibrate and verify the aneroid barometer used in the field to verify the barometric sensors in field. Details are provided in Appendix P. Relative Humidity Calibration Procedure The functioning of the relative humidity calibration is based on the fact that certain salt solutions generate a certain relative humidity in the air above them. The salt solutions suitable for the calibration are lithium chloride LiCl (11% RH) and sodium chloride NaCl (75% RH). For calibration, the sensor head is inserted into a salt chamber containing a saturated salt solution. The probe/transmitter reading is then adjusted to the correct value. Calibration is usually performed with at least two different humidity levels to ensure sensor accuracy over the entire humidity range (0-100% RH). A relative humidity transmitter will be calibrated in the laboratory as a transfer standard for field calibration. Details of the calibration are provided in Appendix E. TEOM 1400 TSP, PM10 and PM2.5 Particulate Monitors Calibration Procedures Procedures are based on routine flow auditing, leak checking, and mass calibration verification. Since the TEOM monitor can be directly mass calibrated, it can be directly quality assured using a mass standard. All QA procedures should be coordinated with routine maintenance procedures to minimize down time. • Flow Audit: A flow audit adapter is provided and the procedures are outlined in the

operating manual. Both the sample flow rate and total flow rate may be checked using the flow audit adapter with a capped nut for closing the flow splitter bypass line port. It is recommended that the volumetric flow rates be within ±7% of the set points. The USEPArequires a tolerance of ±10% for the total flow through the inlet. If measured flow differs by more than the stated tolerances, recheck all settings and perform the test again. Large errors in the flow may indicate other sources of error such as a malfunctioning flow controller, a system leak, or improper temperature and pressure settings. The flow controllers of a TEOM are verified and calibrated by a certified calibrated flow meter. The details of the flow controller calibration are in Section 3.5 of the TEOM service manual.

• Leak Check: The leak check procedures are included in the operating manual (Section 7.6). The leak check is performed with NO sample filter attached to the mass transducer; this

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Page 5 of 6 prevents accidental damage from occurring to the sample filter cartridge when exposed to the high pressure drop (vacuum) in the sample line created by the leak check. Flow rates should indicate less than 0.15 L/min for the main flow and less than 0.65 L/min for the auxiliary flow with the end of the sample line closed; if not, systematically check plumbing for connector leaks.

• Mass Calibration Verification: The mass transducer is permanently calibrated and never requires recalibration under normal use. However, the mass measurement accuracy of the instrument may be verified following procedures in the operating manual. R&P offers a mass calibration verification kit to help perform this procedure. A detailed explanation of how the calibration is performed can be found in Appendix M, N, and O and in Section 3.2.5 in the TEOM service manual.

Instruments for Litter Analysis in Agricultural Waste Management Laboratory The pH electrode is the only laboratory analysis instrument that can be calibrated. Prior to use on any set of samples, the pH electrode is checked with purchased standards at a pH of 4, 7 and 10. The electrode requires calibration when the pH data point “floats” or is out of range (±0.1) from the standard. Reagents used during the analyses are bought or mixed using purchased laboratory grade chemicals. Where required, mixed reagents are standardized as provided in the method (See Appendix S). In place of calibration, the TKN digester and the ammonia distillation apparatus are tested with standards during each sample set using glycine. 100% recovery of the glycine is an indication of proper equipment function. In the event that recovery of less then 98% occurs, the standard will be re-run and then the equipment function will be evaluated to determine the cause of the problem. Results of glycine analysis are recorded with each litter sample set result. 17.3 Calibration Standards Calibration Gas Certifications for calibration gases (NH3, CO2, H2S, CH4 and Propane) are according to EPA Traceability Protocol for Assay & Certification of Gaseous Calibration Standard September 1997, using protocol G1 and or G2, where available for a given concentration. The calibration gas standard is indicated in Table 15.1. All calibration gases need to have a certificate of analysis and cannot be used outside their expiration date. When calibration gases expire, new cylinders are purchased. Flow Rate The flow rate standard apparatus used for flow-rate calibration (field-NIST-traceable, piston-type volumetric flow rate meter; laboratory-NIST-traceable manual soap bubble flow meter and time monitor) has its own certification and is traceable to other standards for volume or flow rate that are themselves NIST-traceable. A calibration relationship for the flow-rate standard, such as an equation, curve, or family of curves, is established by the manufacturer (and verified if needed) that is accurate to within 2% over the expected range of ambient temperatures and pressures at which the flow rate standard is used. The flow rate standard will be recalibrated and recertified at least annually.

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Page 6 of 6 The actual frequency with which this recertification process must be completed depends on the type of flow rate standard; some are more stable than others. The project team will maintain a control chart (a running plot of the difference or percentage difference between the flow rate standard and the NIST-traceable primary flow rate or volume standard) for all comparisons. In addition to providing excellent documentation of the certification of the standard, a control chart also gives a good indication of the stability of the standard. If the two standard-deviation control limits are close together, the chart indicates that the standard is very stable and could be certified less frequently. The minimum recertification frequency is one year. On the other hand, if the limits are wide, the chart indicates a less stable standard that will be recertified more often. Temperature The EPA Quality Assurance Handbook, Volume IV (EPA 1995), Section 4.3.5.1, gives information on calibration equipment and methods for assessing response characteristics of temperature sensors. The temperature standard used for temperature calibration has its own certification and is traceable to a NIST primary standard. A calibration relationship to the temperature standard (an equation or a curve) is established that is accurate to within 2% over the expected range of ambient temperatures at which the temperature standard is to be used. The temperature standard must be reverified and recertified at least annually. The actual frequency of recertification depends on the type of temperature standard; some are much more stable than others. The best way to determine recertification requirements is to keep a control chart. The project team will use an ASTM- or NIST-traceable mercury in glass thermometer, for laboratory calibration. Pressure The Fortin mercurial type barometer works on fundamental principles of length and mass and is therefore more accurate, however, it is more difficult to read and correct than other types. By comparison, the precision aneroid barometer is an evacuated capsule with flexible bellows coupled through mechanical, electrical, or optical linkage to an indicator. It is potentially less accurate than the Fortin type but can be transported with less risk to the reliability of its measurements and presents no damage from mercury spills. The Fortin type of barometer is best employed as a higher quality laboratory standard which is used to adjust and certify an aneroid barometer in the laboratory. 17.4 Document Calibration Frequency

See Table 15.1 for a summary of QC checks that includes frequency and acceptance criteria and references for calibration and verification. All of these events, as well as calibration equipment maintenance are documented in field data records and notebooks and annotated with the flags required in the manufacturer’s operating instruction manual and any others indicated in Section 23 of this document. Laboratory and field activities associated with equipment used by the respective technical staff are kept in record notebooks as well. The records are normally controlled by the managers and located in the labs or field sites when in use or at the manager’s offices when being reviewed or used for data validation.

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12.0 sampling methods requirements - biosystems … detection limit is 0.01 ppm for a 0-10 ppm...

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